تفاعل #2487415

معادلة التفاعل

2-Hydroxyethyl methacrylate

succinic anhydride

Triethylamine

→

liquid

المردود 77.8%

4-(2-(Methacryloyloxy)ethoxy)-4-oxobutanoic Acid

المردود 77.8%

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe reaction mixture was refluxed for 1.5 hours
2. 2
   غسيلwashed with 2 M HCl (150 mL)
3. 3
   أخرىThe organic phase was separated from the aqueous phase
4. 4
   تجفيفdried (MgSO4 and Na2SO4)
5. 5
   أخرىevaporated to dryness

الإجراء التجريبي

2-Hydroxyethyl methacrylate (25 g, 0.195 mol) and succinic anhydride (19.5 g, 0.195 mol) were added to dichloromethane (200 mL) under nitrogen. Triethylamine (28.5 ml, 20.72 g, 1.05 equiv.) was then added dropwise over 20 minutes and the reaction mixture was refluxed for 1.5 hours. The reaction mixture was then diluted with dichloromethane (200 mL), washed with 2 M HCl (150 mL) and then finally with brine (100 mL). The organic phase was separated from the aqueous phase, dried (MgSO4 and Na2SO4) and evaporated to dryness, yielding a viscous, colourless liquid (34.9 g, 77.8% yield). 1H NMR δ 1.89 (s, 3H, CH3), 2.59-2.67 (m, 4H, 2×CH2CO), 4.31 (br. s, 4H, 2×CH2OCO), 5.55 (s, 1H, vinyl CH), 6.08 (s, 1H, vinyl CH). 13C NMR δ 17.96, 28.64, 28.73, 62.15, 62.29, 126.12, 135.79, 167.11, 171.90, 177.73.

المصدر